CHY 42.

1 Exercise 1

Separation/Purification Techniques 1

Distillation and Sublimation

BS BIOLOGY 1BX

ADAJAR, ADAH YLISHA

ARANGGO, RONALDSON II

ATURO, LEAH

BAYNOSA, JOEMARIE

BERBIGAL, CHRIZL

JANUARY 24-27, 2020

 INTRODUCTION

Distillation and Sublimation are both techniques of purification and are used variously
depending on the aim of the experiment, it also varies from the materials available, since
distillation is from liquid to gas and sublimation is heating the solid until its vapour is high
enough to collect on a cooled surface above solid.

I. Distillation

The molecules of the liquid resulting in vapour are seen to form bubbles, which rise
rapidly through the liquid and escape through gaseous state. The boiling point is constant for
identical molecules. This phenomenon is called distillation, which is the basis for purification of
organic compounds. In this process, the liquid organic compound is converted into its vapour
state at its boiling point and by subsequent cooling the vapours is condensed into the liquid state.
In our case, we used an alcoholic beverage that has an 80 proof to distillate. The type of
distillation used in this experiment is simple distillation in which is a large temperature
difference between boiling points of the components to be separated is required to obtain an
efficient separation.

The experiment was conducted with the following objectives:

a.) collect the distilled alcohol from the alcohol beverage

b.) identify he separated alcohol from the mixture

c.) test the alcohol purification from the distillate

II. Sublimation

One technique of purification which the solid is heated until its vapour is high enough to
collect on a cooled surface above solid. This procedure is about the mechanism of evaporation of
molecules or atoms from the solids and with the mechanism of crystal growth from vapours.

The experiment was conducted with the following objectives:

a.) test the percentage of recovery of naphthalene, camphor, and pthalic acid
anhydride using the method of sublimation
 METHODOLOGY

I. Distillation

A. Chemicals and Apparatus

The chemical used in this experiment was 50 mL of Tanduay Rhum with a proof
of 80. The apparatus’s used in this experiment are as follows: (1) 150◦C thermometer with
rubber stopper, (1) 500 mL distilling flask with rubber stopper, (1) condenser with rubber stopper,
(1) glass adapter, (1) hot plate, (3) iron stand, (3) utility clamp, (1) 50mL Erlenmeyer flask, (5)
boiling chips, (1) graduated cylinder, (2) rubber tubing. Below is the picture of the set-up and
how the apparatus are arranged according to its use.

Figure 1. example of simple distillation set-up

B. Procedure

The students measured 50 mL of the alcohol beverage using the graduated

cylinder before pouring the alcohol beverage in the distilling flask, after measuring it is then
poured into the distilling flask and attached into the iron stand using the utility clamp. The
thermometer is then placed in the mouth of the distilling flask to measure the temperature of the
alcohol beverage once it reaches its first boiling point. The bottom of the distilling flask is
position in the hot plate to aid in boiling and 5 boiling chips were added inside the distilling flask
together with the alcohol beverage to help it boil more calmly to avoid accidents. The rubber
tubing is then attached to the condenser and is also attached to the faucet for running water to
cool down the vapour that passes through it. It is also made sure that during the duration of the
experiment all the students wore their personal protective equipment to avoid accidents under the
supervision of the instructor.

II. Sublimation

A. Chemicals and Apparatus

The chemicals used in this experiments are as follows: 2 grams of naphthalene, 2

grams of camphor and 2 grams of pthalic acid anhydride. The apparatus’s used in this
experiment are as follows: (1) watch glass, (1) alcohol lamp, (1) crucible tongs, (1) iron stand, (1)
iron ring, (1) wire gauze. Below is the picture of the set-up and how the apparatus are arranged
according to its use.

Watch glass

Alcohol lamp

Figure 2. Sublimation set-up

 B. Procedure

The students measured 2 grams each of the chemicals using the triple beam
balance; they also separately measured the weight of the watch glass. After weighing the
students immediately proceeded to doing the experiment. The students first cleaned the apparatus
then they lit the fire and heated up the watch glass above the wire gauze before putting
naphthalene in the watch glass. After cleaning, they placed the naphthalene in the watch glass
under the fire and waited for it to dissolve.

C. Mathematical equation

The percentage of recovery of the chemical was calculated using the equation

𝐵
x 100 A= weight of sample of the crude substance B= weight of sample of the sublimate
𝐴
 DATA/RESULTS/CALCULATIONS

I. Distillation

During the experiment the students were tasked to record the temperature when it reaches
its boiling point and the recorded temperature was 74 degrees Celsius. Before the alcohol
beverage was purified, the colour of the mixture was reddish brown and the alcohol proof of the
beverage was 80 proofs and since it is distillation the state of the mixture was liquid. After the
distillation process, the alcohol was separated from the mixture that is called ‘distillate’. The
noticeable changes of the distillate is that it is now colourless, also it gives off a very strong
smell of alcohol and when the students tried to lit it up, it catches fire therefore making it
flammable.

II. Sublimation

The experiment was observed properly and the data were written down carefully that it
wouldn’t misrepresent the result in any way. The students also made sure that during the
conduction of the experiment, no interventions were made to make sure the experiment is a
success and correct data is collected. Everything was executed with the supervision of the
instructor, the students are also wearing their personal protective equipment to make sure of their
safety during the conduction of the experiment. The results of the experiment are summarized
in Table 1 below.

Table 1. Naphthalene in % of recovery

CRUDE SUBSTANCE SUBLIMATE

Wt. Container + sample 27.97 g 28.94 g
Wt. of container 28.98 g 28.61 g
Wt. of sample A= 0.99 g B= 0.33
% of recovery 𝐵
x 100= 33%
𝐴
Table 2. Camphor in % of recovery

CRUDE SUBSTANCE SUBLIMATE

Wt. Container + sample 27.71 g 32.92 g
Wt. of container 26.69 g 32.27 g
Wt. of sample A= 1.03g B= 0.65g
% of recovery 𝐵
x 100= 63%
𝐴

Table 3. Pthalic Acid Anhydride in % of recovery

CRUDE SUBSTANCE SUBLIMATE

Wt. Container + sample 24.99 g 32.92 g
Wt. of container 23.99 g 23.88 g
Wt. of sample A= 1.00 g B= 0.93 g
% of recovery 𝐵
x 100= 93%
𝐴

The percentage of recovery tells you the percentage of an original substance that is
recovered after a chemical reaction is completed, it also determines how efficient the purification
done on the substance. This data will be used for deducting the results and therefore being used
in drawing the conclusion of the experiment.
 DISCUSSION/INTERPRETATION OF RESULTS

I. Distillation
Distillation is a procedure by which two liquids with different boiling points can
be separated, according to Charles D. Schaeffer, Jr., Professor Emeritus of
Elizabethtown College. In this activity the chemical that used was Tanduay Rhum
with 80% proof with a color of reddish-brown. The chemical was then undergone to
the process and the first drop was recorded on 74 degrees Celsius and now colorless.
It was then proved purified after lighting it up with the help of matches.

II. Sublimation
Sublimation is the transition from the solid phase to the gas phase without passing
through an intermediate liquid phase, according to Anne Marie Helmenstine. With the
different chemicals used which are the Naphthalene, Camphor and Pthalic Acid
Anhydride with 2 grams each went to the process of sublimation. After recording the
data needed and solving afterwards the percentage of recovery are the following:
table 1 Naphthalene 33%, table 2 Camphor 63% and table 3 Pthalic Acid Anhydride
93%.